CN105368452A - Silicon oxide layer etching liquid - Google Patents
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Abstract
The invention relates to a silicon oxide layer etching liquid, which comprises fluorine compounds, sulfonic compounds comprising at least two sulfuric radicals, salts of the sulfonic compounds, and water. The provided etching liquid can maintain the etching speed on silicon oxide layer, and at the same time, reduces the etching speed on silicon nitride layer, which is taken as the lower insulation membrane of the pixel electrode. So the loss of the nitride layer is minimized, and the lower membrane is protected. A thinner nitride layer structure becomes feasible. The defects during the process of semiconductor production are reduced, and a finer semiconductor structure can be formed.
Description
Technical field
The present invention relates to silicon oxide layer etching solution, especially relate to, to silicon oxide layer, there is high optionally silicon oxide layer etching solution.
Background technology
In the component manufacturing process of semiconductor structure, the electrical isolation between metallic substance during for realizing between plain conductor and forming grid (Gate) and source/drain (S/D), uses silicon oxide layer (SiO
2) and silicon nitride layer (SiN
x).Silicon oxide layer and silicon nitride layer can according to Processes and apparatus for different objects.
In semi-conductor or thin layer display fabrication process, when forming circuit substrate, the hardware for realizing grid (Gate) and source/drain (Source/Drain) electrical isolation and in the silicon oxide layer formed, for the contact hole (Contacthole) needed for the formation of formation contacting metal (Contactmetal), due to the purposes of its etching part silicon oxide layer, can use and comprise hydrogen fluoride (HF) and Neutral ammonium fluoride (NH
4f) etching solution (buffered oxide etch agent).
When the silicon oxide layer etching of this type of routine, use under the state directly do not exposed to the open air at hardware or between zone of oxidation and metal level, there is blocking layer state under use, and can't directly to have an impact to metal level.But when generally silicon nitride layer being used as blocking layer, major part exposes to the open air simultaneously.
Therefore, the purposes of silicon nitride layer is the formation for the protection or patterned layer maintaining etching mask or metal level, thus need not with silicon oxide layer simultaneously etched characteristic.For these reasons, need the composition for silicon nitride layer with the larger etching selectivity to silicon oxide layer, can expect indirectly protected effect to metal and metal pattern layer.
Generally speaking, as the method increased relative to the etching selectivity of the silicon oxide layer of silicon nitride layer, the method for the etching speed increasing silicon oxide layer or the etching speed reducing silicon nitride layer can be used.Usually, by HF and NH
4when F forms etch combination, there is following characteristic: when silicon oxide layer etching speed increases, the etching selectivity of silicon oxide layer is also increased simultaneously.But, for the etching speed of silicon oxide layer, according to use and processing condition, equipment (device) kind, require to the silicon oxide layer etching speed be fixed, therefore, need following method: while the etching speed maintaining silicon oxide layer, reduce the etching speed of silicon nitride layer.
The etching solution high to the Selection radio of silicon oxide layer can be applied to the etching for carrying out the variation of the element according to semiconductor design rule (designrule) and the pattern of complex construction and cleaning, and in process for manufacture of semiconductor device, when silicon oxide layer is had the fine pattern of high integration as mask formation, can be used in the selective etch technique of silicon oxide layer.
In order to increase the etching selectivity of silicon oxide layer, implement to utilize additive optionally to reduce the research of the etching speed of nitride layer.As an example, in Korean Patent Application No. 10-2004-0034566, disclose the composition utilizing alkylsurfuric acid salt (such as ammonium lauryl sulfate) additive.In addition, Korean Patent Application No. 10-2009-0075542 discloses the composition utilizing polyxyethylated ammonium sulfate (ammoniumpolyoxyethylenealkylsulphate), and Korean Patent Application No. 10-2009-0063235 discloses the anionic polymer additive of such as poly-sulfonic acid or polyacrylic acid/sulfonic acid copolymer.But, above-mentioned composition fully cannot realize the Selection radio of zone of oxidation/nitride layer required in semiconductor technology, or the solubleness because of liquid etching composition is not enough and cause technologic problem, or in high molecular situation, the defects (defect) such as additive remains may be there is because forming Macromolecule aggressiveness in fine pattern treatment process.
Therefore, need to develop the selective etch composition that can realize the silicon oxide layer of outstanding performance in following: additive solubleness, Selection radio improve effect, defect occurs minimized.
Summary of the invention
Technical problem
Problem to be solved by this invention for providing silicon oxide layer etching solution, to solve the problem.
Technique means
For solving above-mentioned problem, the invention provides the silicon oxide layer etching solution comprising following composition:
Fluorine cpd;
The sulfoacid compound of following chemical formula 1 or its salt; And
Water;
[chemical formula 1]
In above-mentioned chemical formula 1, A is the straight or branched organic group of C1 to C60 or the alicyclic or aromatic organic radicals of C4 to C60, and x is the integer of more than 2; And
The molecular weight of the sulfoacid compound of above-mentioned chemical formula 1 is not more than 1000.
Invention effect
Silicon oxide layer etching solution of the present invention has the improvement effect of following aspect: higher silicon oxide layer etching speed, and has the higher Selection radio to silicon oxide layer for silicon nitride layer.Thus, will the damage of silicon nitride layer be suppressed in semi-conductor and display processes, thus the defect of etching mask layer or metal level or minimizing patterned layer can be protected, and make it possible to use thinner silicon nitride layer, meticulous pattern can be formed.
Embodiment
The present invention can carry out various distortion and can have numerous embodiments, next will be described in detail in embodiment part to specific embodiment.But, do not intend the present invention to be limited to specific embodiment, the present invention can be understood and comprise all distortion fallen in spirit and scope of the invention, equivalent and surrogate.In following description of the present invention, if think the specific descriptions of relevant known technology are an impediment to and theme of the present invention is understood, then will description is omitted.Below, the present invention will be described in more detail.
The present invention relates to the silicon oxide layer etching solution high for silicon oxide layer selectivity.
Silicon oxide layer etching solution of the present invention comprises: fluorine cpd, has sulfonic sulfonic acid or the sulfonate compound of more than 2, water, and optionally comprise mineral acid, organic acid or its mixture in molecule.
Silicon oxide layer etching solution of the present invention comprises the sulfonic sulfonic acid or sulfonate compound with more than 2, while maintaining the etching speed of silicon oxide layer, reduces the etching speed of silicon nitride layer, play the effect of protection silicon nitride layer at fluorine cpd.
As a result, silicon oxide layer etching solution of the present invention not only has high etching speed to silicon oxide layer, and provide the Selection radio to silicon oxide layer increased for silicon nitride layer by reducing the etching speed of silicon nitride layer, thus optionally etching silicon oxide layer.
Sulfonic sulfonic acid or the sulfonate compound with more than 2 represent by following chemical formula 1:
[chemical formula 1]
In above-mentioned chemical formula 1, A is the straight or branched organic group of C1 to C60 or the alicyclic or aromatic organic radicals of C4 to C60, and x is the integer of more than 2;
The molecular weight of the sulfoacid compound of above-mentioned chemical formula 1 is not more than 1000.
Preferably, A represents the alicyclic of C12 to C24 or aromatic series, and x is the integer of 2 to 10, and total molecular weight can be less than 600.
The specific examples of the sulfoacid compound represented by chemical formula 1 can be the compound of following chemical formula 2 to chemical formula 7.
[chemical formula 2]
[chemical formula 3]
[chemical formula 4]
[chemical formula 5]
[chemical formula 6]
[chemical formula 7]
In above-mentioned chemical formula, R
2and R
3can be independently of one another hydrogen atom or C1 to C20 alkyl or for the alkyl of C1 to C14 or the alkyl of C1-C6, and can to exist with one or more;
M and n is the integer of more than 2 independently of one another;
P and q is the integer of more than 0 or 1, and p+q is the integer of more than 2.
Preferably, m, n and p+q can be the integer of 2 to 10 independently of one another.
The preferred embodiment of sulfoacid compound can be selected from: Alkylene disulfonic, polyalkylbenzene sulfonic acid, alkyl biphenyl ether disulfonic acid, alkyl sulfonyl phenoxyl benzene disulfonic acid, alkyl sulfonyl phenoxyl benzene trisulfonic acid, alkylnaphthalene disulfonic acid, alkylamino naphthalene disulfonic acid and their salt etc.
Salt can be selected from lower group one or more: the sodium salt (Na of sulfonic acid
+), sylvite (K
+), molysite (Fe
2+), calcium salt (Ca
2+) or ammonium salt (NH
4 +) etc., but be not limited to this.
Relative to the silicon oxide layer etching solution that gross weight is 100 parts, the compound or its salt of above-mentioned chemical formula 1 can be 0.001 to 5 weight part, is preferably 0.001 to 3 weight part or 0.005 to 1 weight part.
In the present invention, fluorine cpd can be used as the etching composition of silicon oxide layer, described fluorine cpd can use be selected from hydrofluoric acid (HF) or hydrofluoride one or more.
In the present invention, representational hydrofluoride can use and be selected from Neutral ammonium fluoride (NH
4f), fluoram (NH
4hF
2) in one or more, but be not limited to this, as long as known in the art all can use and unrestricted.
Relative to the silicon oxide layer etching solution that gross weight is 100 parts, 0.01 to 60 weight part can be comprised, preferably can comprise the fluorine cpd of 5 to 50 weight parts or 10 to 40 weight parts.
In the present invention, when using hydrofluoride, being the silicon oxide layer etching solution of 100 parts relative to gross weight, 1 to 40 weight part can be comprised, preferably can comprise the hydrofluoride of 5 to 30 weight parts or 10 to 30 weight parts.
In the present invention, silicon oxide layer etching solution also can comprise mineral acid, organic acid and their mixture further as sour composition.
As mineral acid, can be selected from lower group one or more: phosphoric acid, hydrochloric acid, sulfuric acid, nitric acid, hydroperoxy acid or boric acid.
As organic acid, can be selected from lower group one or more: formic acid, acetic acid, oxalic acid, iminodiethanoic acid, methylsulfonic acid, ethyl sulfonic acid, lactic acid, xitix, oxalic acid or citric acid, as long as but known in the art all can use and unrestricted.
Mineral acid and organic acid can be used alone, but also can be used in combination.
Relative to the silicon oxide layer etching solution that gross weight is 100 parts, 0.01 to 60 weight part can be comprised, preferably can comprise independent mineral acid, organic acid or its mixture of 1 to 30 weight part, within the scope of this, fully can realize the effect that silicon oxide layer is etched.According to an embodiment, by regulating mineral acid, the concentration of organic acid or its mixture and Neutral ammonium fluoride carrys out the etching speed of controlled oxidization silicon layer.
The water be contained in silicon oxide layer etching solution has no particular limits, and can use deionized water, preferably can use the deionized water that the ratio resistance value of water (representing the ion remaval degree in water) is 18M Ω/more than cm.The content of water makes the gross weight of composition be the residual content of 100 parts.
In the present invention, silicon oxide layer etching solution also can comprise tensio-active agent further, adds tensio-active agent further to improve the wetting property of silicon oxide layer etching solution, to improve the foam characteristic of additive
and the solvability improved other organic additive.Tensio-active agent can be selected from nonionogenic tenside, anion surfactant, cats product, amphoterics one or more, and be the etching solution of 100 parts relative to gross weight, 0.0005 to 5 weight part can be added, be preferably the etching solution of 100 parts relative to gross weight, 0.001 to 2 weight part can be added.When the content of tensio-active agent is lower than 0.0005 weight part for the gross weight of etching solution, cannot tells on, and when interpolation is greater than 5 weight part, solubility will be caused or cause technologic problem because producing too much foam.
As long as the tensio-active agent be dissolved in silicon oxide layer etching solution of the present invention can use and without any restrictions, such as, the kinds of surface promoting agents such as polyalkylene oxides alkyl phenyl ethers tensio-active agent, alkyl carboxylic acid, alkyl sulfuric ester, alkylsulphonic acid, alkyl benzene sulphonate (ABS), alkylamine, imidazolines can be used, but be not limited to the above-mentioned tensio-active agent enumerated.
According to the present invention, in order to protection is used as metal or the metallic compound of semiconductor element material when processing with etching solution, antioxidant and anticorrosive agent can be added in silicon oxide layer etching solution.As long as can adopting of using in antioxidant and the anticorrosive agent industry and unrestricted, and for the etching solution that gross weight is 100 parts, 0.01 to 10 weight part can be added.
As the example of antioxidant and anticorrosive agent, can to be selected from lower group one or more: the mercaptan compounds such as halfcystine, Thiovanic acid, cysteamine, xitix, aromatic heterocyclic compounds, aliphatic heterocycle, aromatic series multivalence alcohol and branched structure multivalence alcohol.Representational aromatic heterocyclic compounds ground can be selected from furans, thiophene, pyrroles, oxazole, thiazole, imidazoles, pyrazoles, triazole, tetrazolium, benzotriazole, benzoglyoxaline, amino tetrazole, methyl tetrazolium, tolytriazole, hydroxytoluene triazole, and representational aliphatic heterocycle can be selected from piperazine, methylpiperazine, hydroxyethylpiperazin.
According to the present invention, silicon oxide layer etching solution also can comprise organic solvent further.As above-mentioned tensio-active agent, organic solvent improves wettability and improves the solubleness of organic additive or can be used as solvent and partly or entirely substitute water in liquid etching composition, in this case, make it possible to improve the stability in storage of product under low-temperature storage.
Organic solvent can be alcohols.Specifically, can be and be selected from following one or more: methyl alcohol, ethanol, propyl alcohol, ethyl glycol, ethyl Diethylene Glycol, ethyl triethylene glycol, butyl diglycol, polyoxyethylene glycol and polypropylene glycol.
Relative to the etching solution that gross weight is 100 parts, the organic solvent of below 10 weight parts can be comprised.
Silicon oxide layer etching solution described in above-mentioned embodiment makes by following method.
In one embodiment, the method manufacturing silicon oxide layer etching solution can comprise the steps: by fluorine cpd and water being carried out mixing manufacturing the aqueous solution; And, in this aqueous solution, add the compound or its salt of chemical formula 1; And, the step of adding mineral acid, organic acid or its mixture can be comprised as required.
In above-mentioned manufacture method, as described above, and the example also as described above: fluorine cpd for the content of following material; Mineral acid, organic acid or its mixture; The compound or its salt of chemical formula 1; And water.
Above-mentioned manufacture method can comprise the step of adding and being selected from one or more following additives as required: tensio-active agent, antioxidant, anticorrosive agent and organic solvent.
Above-mentioned manufacture method is by holding quantitative limitation, be applicable to a small amount of production and produce in a large number, in addition, the temperature and the pressure that can be used for manufacturing above-mentioned etching solution are not also particularly limited, but normal temperature can be used (such as, 20 to 25 DEG C) and the condition of normal pressure (such as, 1 normal atmosphere).
Silicon oxide layer etching solution of the present invention can be used for the etch process of the zone of oxidation in process for manufacture of semiconductor device.
That is, the silicon oxide layer etching solution described in the application of the invention, implements the step of protection silicon nitride layer and optionally etching silicon oxide layer in the manufacturing process of semiconductor structure element, makes it possible to manufacture semiconductor element.
Below, will be described in detail to embodiments of the present invention, easily implement the present invention to help those skilled in the art.But the following example is only and the present invention is shown, and content of the present invention can't be limited to following embodiment.
Embodiment and comparative example
Manufacture silicon oxide layer etching solution to evaluate etching speed.The implication of the shortenings used in following embodiment and comparative example is as follows:
AA: acetic acid (aceticacid);
ADPDS: alkyl (C12) diphenyl oxide disulfonic acid (dodecyl-(sulfophenoxy) Phenylsulfonic acid);
PSS: polystyrolsulfon acid (polystyrenesulfonicacid; Weight average molecular weight is 800);
ANDS: alkyl (C10) naphthalene disulfonic acid (decyl naphthalene disulfonic acid);
ABDS: alkyl (C10) benzene disulfonic acid (decyl benzene disulfonic acid);
ABPDS: alkyl (C10) biphenyl disulfonic acid (decyl biphenyl disulfonic acid);
AANDS: alkyl (C10) amino naphthalenes disulfonic acid (aminodecyl naphthalene disulfonic acid);
ABS: alkyl (C12) phenyl-hydrogen-sulfate ester (dodecylbenzene sulfuric ester);
AS: alkyl (C8) sulfuric ester (octyl sulfate ester);
AD: nonionogenic tenside (acetylenediol);
ATZ: anticorrosive agent (amino tetrazole).
Prepare silicon oxide layer etch combination (1)
Each composition of the component content had shown by following table 1 is mixed, manufactures silicon oxide layer etching solution.The content of water is the residual content making the gross weight of composition reach 100wt%.
Table 1
Prepare silicon oxide layer etch combination (2)
Each composition of the component content had shown by following table 2 is mixed, manufactures silicon oxide layer etching solution.The content of water is the residual content making the gross weight of composition reach 100wt%.
Table 2
Experimental example 1: the evaluation of silicon oxide layer etching speed
On Silicon Wafer respectively with
thickness form silicon oxide layer (thermal oxide) and silicon nitride layer (SiN
x) after, by cutting the sample of each sample making layer thickness measurement with the size of 20mm × 30mm.
Contactless layer thickness measuring instrument (ST-2000DLXn, K-MAC company) is used to carry out layer thickness measurement.Silicon oxide layer (thermal oxide) and silicon nitride layer (SiN
x) layer thickness evaluation method be: 100g silicon oxide layer etching solution is loaded after transparent plastic container, utilizes constant temperature circulating groove that temperature is adjusted to 25 DEG C, according to etching speed regulating time, the evaluation sample measured for layer thickness is etched.The etching speed of silicon oxide layer and silicon nitride layer is converted into based on the treatment time with unit
represent.
Table 3
Table 4
According to the result of above-mentioned table 3 and table 4, compared to the comparative example with corresponding composition, silicon oxide layer etching solution described in embodiments of the invention 1 to embodiment 12 demonstrates following result: while the etching speed maintaining silicon oxide layer, and the etching speed of silicon nitride layer reduces.From the above results, compared with the comparative example with identical etching speed, the silicon oxide layer etching solution described in embodiments of the invention 1 to embodiment 12 has for the etching speed Selection radio of silicon oxide layer/silicon nitride layer the effect improving more than 2-3 times.
In addition, the silicon oxide layer etching solution of comparative example 6 because of added 0.01% the low solubleness of alkyl (C12) phenyl-hydrogen-sulfate ester, cannot evaluate the etching of sample, in addition, in the comparative example 7 of another alkyl as sulfate compound additive (C8) sulfuric ester of interpolation 0.2%, although there is not the problem that solubleness reduces, do not observe the improvement effect of etching selectivity.
Therefore, when using silicon oxide layer etching solution of the present invention, from the substrate of the manufacture semi-conductor and indicating meter that are mixed with silicon nitride layer and silicon oxide layer, only optionally can remove silicon oxide layer, thus the defective workmanship that the damage because of silicon nitride layer can be made to cause is minimized.
Claims (12)
1. one kind comprises the silicon oxide layer etching solution of following composition:
Fluorine cpd;
The sulfoacid compound of following chemical formula 1 or its salt; And
Water;
[chemical formula 1]
In described chemical formula 1, A is the straight or branched organic group of C1 to C60 or the aliphatics of C4 to C60 or aromatic organic radicals, and x is the integer of more than 2;
The molecular weight of the sulfoacid compound of described chemical formula 1 is not more than 1000.
2. silicon oxide layer etching solution according to claim 1, is characterized in that, described fluorine cpd be selected from hydrofluoric acid and hydrofluoride one or more.
3. silicon oxide layer etching solution according to claim 2, is characterized in that, described hydrofluoride be selected from Neutral ammonium fluoride and fluoram one or more.
4. silicon oxide layer etching solution according to claim 1, wherein, the compound of described chemical formula 1 is the compound of following chemical formula 2 to chemical formula 7:
[chemical formula 2]
[chemical formula 3]
[chemical formula 4]
[chemical formula 5]
[chemical formula 6]
[chemical formula 7]
In above-mentioned chemical formula,
R
2and R
3be the alkyl of hydrogen atom or C1 to C20 independently of one another, and can exist with one or more;
M and n is the integer of more than 2 independently of one another;
P and q is the integer of more than 0 or 1, and p+q is the integer of more than 2.
5. silicon oxide layer etching solution according to claim 4, wherein, in described chemical formula, m, n and p+q are the integer of 2 to 10 independently of one another.
6. silicon oxide layer etching solution according to claim 1; it is characterized in that, the compound of described chemical formula 1 is selected from: the salt of Alkylene disulfonic, polyalkylbenzene sulfonic acid, alkyl biphenyl ether disulfonic acid, alkyl sulfonyl phenoxyl benzene disulfonic acid, alkyl sulfonyl phenoxyl benzene trisulfonic acid, alkylnaphthalene disulfonic acid, alkylamino naphthalene disulfonic acid and these sulfonic acid.
7. silicon oxide layer etching solution according to claim 1, is characterized in that, described salt is sodium salt, sylvite, molysite, calcium salt or ammonium salt.
8. silicon oxide layer etching solution according to claim 1, wherein, the silicon oxide layer etching solution of 100 weight parts comprises:
The fluorine cpd of 0.01 to 60 weight part;
The sulfoacid compound of the above-mentioned chemical formula 1 of 0.001 to 5 weight part or its salt; And
The water of residual content.
9. silicon oxide layer etching solution according to claim 1, is characterized in that, described etching solution also comprises organic acid, mineral acid or their mixture further.
10. silicon oxide layer etching solution according to claim 9, is characterized in that, described mineral acid is phosphoric acid, hydrochloric acid, sulfuric acid, nitric acid, hydroperoxy acid or boric acid.
11. silicon oxide layer etching solutions according to claim 9, is characterized in that, described organic acid is formic acid, acetic acid, oxalic acid, iminodiethanoic acid, methylsulfonic acid, ethyl sulfonic acid, lactic acid, xitix, oxalic acid or citric acid.
12. silicon oxide layer etching solutions according to claim 1, is characterized in that, described etching solution also comprise in tensio-active agent, antioxidant and anticorrosive agent further one or more.
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|---|---|
| KR102242951B1 (en) | 2021-04-22 |
| KR20160019878A (en) | 2016-02-22 |
| CN105368452B (en) | 2019-02-19 |
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